CN112723421B - FeMnS x Nanosheet cluster and preparation method thereof - Google Patents

FeMnS x Nanosheet cluster and preparation method thereof Download PDF

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CN112723421B
CN112723421B CN202110151238.4A CN202110151238A CN112723421B CN 112723421 B CN112723421 B CN 112723421B CN 202110151238 A CN202110151238 A CN 202110151238A CN 112723421 B CN112723421 B CN 112723421B
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femns
preparation
clusters
nano
cluster
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CN112723421A (en
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钟晓聪
王瑞祥
徐志峰
林振聪
袁远亮
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Jiangxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/12—Sulfides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/009—Compounds containing, besides iron, two or more other elements, with the exception of oxygen or hydrogen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Abstract

The invention discloses FeMnS x Nanosheet clusters and a preparation method thereof. The FeMnS x The nano-cluster is a cluster formed by FeMnS x The nanoplatelets are stacked into clusters.The preparation method comprises the following steps of firstly, mixing the raw materials in a molar ratio of 1:2, evenly mixing choline chloride and ethylene glycol to obtain a eutectic solvent, and sequentially adding FeCl 3 、MnCl 2 Thioacetamide, urea; then pouring the solution into a hydrothermal reaction kettle, and reacting for 20 hours at 170 ℃; finally, after the reaction kettle is naturally cooled to room temperature, carrying out centrifugal separation, washing and freeze drying to obtain FeMnS x Nanosheet clusters. The FeMnS x The nano-sheet cluster has the advantages of large specific surface area and high catalytic activity of oxygen evolution reaction, and has good commercial application prospect.

Description

FeMnS x Nanosheet cluster and preparation method thereof
Technical Field
The invention relates to the field of nano materials, in particular to FeMnS x A method for preparing a nano-sheet cluster.
Background
The transition metal sulfide has the advantages of abundant raw material reserves, low cost, greenness, no toxicity and high catalytic activity of oxygen evolution reaction, and is widely applied to the field of hydrogen production by water cracking. At present, the transition metal sulfides reported in the literature for oxygen evolution reaction are mainly CoS and NiFeS x 、NiCoS x And CoNiS x And the like. Transition metal sulfides with different compositions and structures can be prepared by changing the metal types and the synthesis method. At present, the common preparation methods of transition metal sulfides mainly comprise a hydrothermal method or a solvothermal method, such as reaction at high temperature of a system of aqueous solution, alcoholic solution and the like to obtain a nano material.
Disclosure of Invention
The invention mainly aims to provide FeMnS x A nanosheet cluster and a preparation method thereof aim to develop an electrocatalyst with large specific surface area and high oxygen evolution activity and a preparation method thereof, improve the oxygen evolution activity of transition metal sulfides, and overcome the defect that a nanometer product is easy to agglomerate in the preparation process of the traditional hydrothermal and solvothermal methods.
In order to achieve the above object, the present invention provides a FeMnS x Nanosheet cluster consisting of FeMnS x Stacking of nanosheets into clusters。
In order to achieve the aim, the invention provides FeMnS x The preparation method of the nanosheet cluster comprises the following steps:
mixing a mixture of 1:2, evenly mixing choline chloride and ethylene glycol at 70 ℃ to obtain a eutectic solvent, and sequentially adding FeCl 3 、MnCl 2 Thioacetamide and urea, wherein FeCl 3 、MnCl 2 The concentration of the compound is 0.25M, and the concentration of thioacetamide and urea is 0.1M;
pouring the solution into a hydrothermal reaction kettle, and reacting for 20 hours at 170 ℃;
after the reaction kettle is naturally cooled to room temperature, centrifugally separating, washing, freezing and drying to obtain FeMnS x Nanosheet clusters.
The basic idea and technical principle of the invention are as follows:
CoS、NiFeS x 、NiCoS x and CoNiS x The transition metal sulfide has good oxygen evolution catalytic activity. Mn is used as a polyvalent metal, and the compound of Mn is an ideal oxygen evolution reaction catalyst. Therefore, the invention tries to introduce manganese into transition metal sulfide, and invents FeMnS for catalyzing oxygen evolution reaction x 。
The common preparation method of the transition metal sulfide mainly comprises a hydrothermal method or a solvothermal method, and the nano material is obtained by adopting an aqueous solution and an alcohol solution and reacting at a high temperature. The solvent adopted in the synthesis process has obvious influence on the composition, crystallinity and morphological structure of the product, so the invention provides the eutectic solvent prepared by choline chloride-ethylene glycol, and FeMnS is obtained by reaction in a reaction kettle x Nanosheet clusters.
The FeMnS is prepared by taking ferric chloride and manganese chloride as metal sources, taking thioacetamide as a sulfur source and taking a low-eutectic solvent prepared from choline chloride and ethylene glycol as a reaction solvent through reaction at a high temperature x Nanosheet clusters. FeMnS x Large specific surface area, high oxygen evolution reaction activity and good application prospect.
Compared with the prior art, the invention has the following beneficial effects:
1) Provides a FeMnS x The nano-sheet cluster has large specific surface area and high oxygen evolution activity;
2) The FeMnS with a unique shape and structure is prepared by adopting a eutectic solvent prepared from choline chloride-ethylene glycol x 。
3) FeMnS prepared using deep eutectic solvent x The nano-cluster has good dispersibility and is not easy to agglomerate.
Drawings
FIG. 1 shows FeMnS in the examples x A topography of the nanoplatelet clusters.
Detailed Description
The present invention will be described in detail with reference to the following examples.
The eutectic solvent is prepared by uniformly stirring choline chloride and ethylene glycol according to a molar ratio of 1. Adding 10mmol of FeCl 3 And 10mmol of MnCl 2 Dissolved in 40mL of the eutectic solvent. 4mmol of thioacetamide and 4mmol of urea are added in sequence and mixed with the eutectic solvent uniformly. The solution prepared above was put into a 100mL hydrothermal reaction kettle and reacted at 170 ℃ for 20h. After the reaction kettle is naturally cooled, the solution in the reaction kettle is centrifugally washed by deionized water and ethanol. Putting the washed sample into a freeze drying box for drying to obtain FeMnS x The morphology of the nanosheet clusters is shown in FIG. 1. FeMnS is treated x Dispersing in ethanol containing Nafion, making into ink, and dripping on foamed nickel of 10mm × 10mm, feMnS x The loading capacity is 1mg/cm 2 . In a 1M KOH solution, the current density was 10mA/cm -2 At 25 deg.C, the oxygen evolution overpotential is about 280mV.

Claims (1)

1. FeMnS x The preparation method of the nano-sheet cluster is characterized in that the FeMnS x The nano-sheet cluster consists of FeMnS x The nano sheets are piled into clusters, and the preparation method comprises the following steps:
mixing a mixture of 1:2, evenly mixing choline chloride and ethylene glycol at 70 ℃ to obtain eutectic solvent, and sequentially adding FeCl 3 、MnCl 2 Thioacetamide, urea, wherein FeCl 3 、MnCl 2 The concentration of the compound is 0.25M, and the concentration of thioacetamide and urea is 0.1M;
pouring the solution into a hydrothermal reaction kettle, and reacting for 20 hours at 170 ℃;
after the reaction kettle is naturally cooled to room temperature, centrifugally separating, washing, freezing and drying to obtain FeMnS x Nanosheet clusters.
CN202110151238.4A 2021-02-03 2021-02-03 FeMnS x Nanosheet cluster and preparation method thereof Active CN112723421B (en)

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RU2256618C1 (en) * 2003-12-08 2005-07-20 Научно-исследовательское учреждение Институт физики им. Л.В. Киренского Сибирского отделения РАН Method for producing ferromagnetic iron-manganese sulfide with giant magnetic resistance
JP2007069270A (en) * 2005-09-02 2007-03-22 Institute Of Physical & Chemical Research Inorganic nanoparticle with high dispersibility
RU2435734C2 (en) * 2010-02-01 2011-12-10 Учреждение Российской академии наук Институт физики им. Л.В. Киренского Сибирского отделения РАН Monocrystalline giant magnetostrictive iron-manganese sulphide
WO2013029186A1 (en) * 2011-09-01 2013-03-07 Trudel Simon Electrocatalytic materials and methods for manufacturing same
CN102751489B (en) * 2012-06-29 2015-04-15 上海交通大学 Method for preparing anode material of lithium ion battery
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